CN103447015A - Desorption and regeneration method for organic matter adsorbent - Google Patents
Desorption and regeneration method for organic matter adsorbent Download PDFInfo
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- CN103447015A CN103447015A CN2013103155052A CN201310315505A CN103447015A CN 103447015 A CN103447015 A CN 103447015A CN 2013103155052 A CN2013103155052 A CN 2013103155052A CN 201310315505 A CN201310315505 A CN 201310315505A CN 103447015 A CN103447015 A CN 103447015A
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Abstract
The invention discloses a desorption and regeneration method for an organic matter adsorbent. The method is characterized in that an organic matter adsorbent desorption and regeneration device of a microwave generator is arranged in a desorption tower; the to-be-desorbed adsorbent with organic matters is put in the desorption tower; steam is aerated from the top of the desorption tower; the microwave generator is started, wherein the microwave power is 500-10000W; desorption is carried out for 2-30 minutes; the desorbed organic matters and steam flow out from a steam outlet at the bottom of the desorption tower and enter a condenser for condensation; then the steam is cut off, nitrogen is aerated from the top of the desorption tower, and the nitrogen flows out from the bottom, wherein the microwave power is 200-2000W; drying treatment is carried out for 2-20 minutes; the microwave generator is turned off, and the nitrogen is cut off; the desorbed adsorbent is obtained. According to the method, the desorption rate is improved by a large margin by combining steam and the microwave technology, and less desorption residue is left.
Description
(1) technical field
The present invention relates to a kind of renovation process of Adsorption of Organic agent, especially the regeneration desorption in active carbon, molecular sieve and macromolecule resin adsorbent for organic molecule, solve current organic exhaust gas, the organic wastewater absorption problem of adsorbent reactivation afterwards.
(2) background technology
Adsorption technology is widely used in organic exhaust gas and organic wastewater improvement at present, and especially, for organic exhaust gas and the waste water of some low concentrations, absorption can be removed organic pollution well, reaches the purpose of purification.In addition, by desorption, recycle, also can realize the recycling of organic pollution.Industrial modal adsorbent has active carbon, NACF, zeolite molecular sieve and high-molecular porous resin etc. at present, and these adsorbents all show good characterization of adsorption.But in organic contamination is processed, except requiring adsorbent, have high efficiency of additive capability, require equally the regenerability that adsorbent can be good, so desorption is also the key technology that organic pollution purifies.The more desorption technology of research has at present: solvent elution, hot-air desorption and steam desorption technology etc., but solvent elution and hot-air desorption easily cause the secondary pollution of subsequent treatment, and organic matter can't be realized the utilization of resources.Therefore in the organic matter desorption reclaims, what obtain extensive use the most is the steam desorption technology.Conduct heat by a large amount of high-temperature vapors, make to adsorb organic molecule and be subject to thermal desorption, be converted into liquid in subsequent condensation together with steam, thereby realizing organic recovery.
But, in industrial practice, there are several problems equally in the steam regeneration techniques: (1) utilizes the agent of steam temperature heating adsorption, consume a large amount of steam; (2) the steam heat from be delivered in the adsorbent duct, and the adsorbent thermal conductance coefficients such as molecular sieve and resin are little, heat transfer rate is slow, desorption time is long; (3) hydrone can be residual in adsorbent, and adsorbent needs hot-air to carry out drying, and energy consumption is higher; (4) desorption product moisture content is high, with separating, brings difficulty to subsequent storage.
For further improving desorption rate, the micro wave regeneration technology becomes study hotspot in recent years, pass through microwave action, can make active carbon heat up rapidly, thereby make to be adsorbed on the quick desorption of surperficial organic molecule, greatly reduce desorption time, and, by subsequent condensation, obtain comparatively single organic liquid product.But Microwave Treatment is having some limitations property equally also: (1) is the medium of the high-k such as Microwave Treatment active carbon at first, easily produces localized hyperthermia and spark, has serious potential safety hazard, and can destroy sorbent structure; (2) with respect to adsorbent (as the zeolite molecular sieve of resin, high hydrophobicity) and the nonpolar adsorbate (benzene, toluene) of high hydrophobicity, because dielectric constant is low, microwave almost can not heat these media, therefore can not reach good desorption effect.
Therefore in the urgent need to a kind of new desorption and regeneration technology, not only use safe and efficiently, and can adapt to adsorbent and the adsorbate of opposed polarity, reclaim the organic matter that obtains low-water-content.
(3) summary of the invention
The purpose of this invention is to provide a kind of new adsorbent surface organic matter desorption technology, can improve desorption rate, reduce energy consumption, and the load separated that reduces organic matter and water.
For achieving the above object, the technical solution used in the present invention is:
A kind of desorption process for regenerating of Adsorption of Organic agent, described method is: in desorption column, be provided with in the desorption and regeneration device of Adsorption of Organic agent of microwave generator, there is organic adsorbent to be placed in desorption column the absorption for the treatment of desorption, pass into steam from desorption column top vapour inlet, open microwave generator, microwave power 500-10000W, carry out desorption and process 2～30 minutes, the organic matter of desorption and steam flow out from desorption column bottom vapor outlet port, enter condenser condenses; Then cut off steam, from desorption column top nitrogen inlet, pass into nitrogen, the bottom nitrogen outlet flows out nitrogen, and microwave power is 200-2000W, carries out drying processing 2-20 minute, stops microwave generator and cuts off nitrogen, obtains the adsorbent after desorption.
Described microwave power can be regulated according to adsorption tower inner volume size, makes the whole adsorption tower of microwave field stepless action.
The 0.2-5.0 that the volume that described steam per hour passes into is the adsorbent volume doubly, suitably regulate according to the adsorbent dielectric constant is different by its consumption.
The air speed of described nitrogen is 500-5000h
-1, be preferably 2000h
-1.
The present invention also provides a kind of desorption and regeneration device of Adsorption of Organic agent, described device comprises desorption column, steam generator, nitrogen gas generator, condenser, and be located at the microwave generator in desorption column, described steam generator is communicated with the vapour inlet on desorption column top by flowmeter, nitrogen gas generator is connected with the nitrogen inlet on desorption column top by flowmeter, nitrogen outlet and vapor outlet port are located at respectively the desorption column bottom, and vapor outlet port is communicated with condenser.
Can load the adsorbent for the treatment of desorption in desorption column, described adsorbent can be the various adsorbable organic adsorbents such as active carbon, NACF, zeolite molecular sieve, high-molecular porous resin.Steam generator is regulated the steam flow by flowmeter, and nitrogen gas generator is regulated nitrogen flow by flowmeter.
Described device can connect a storage container in condensator outlet, organic matter and the water of the liquid state that storage condenses from condenser.
The operation principle of desorption technology of the present invention is as follows: steam generator produces a certain amount of water vapour, steam is passed into desorption column, open the microwave generator of desorption column inside, make microwave field evenly make in whole desorption column, steam, under microwave action, had both prevented water vapor condensation, can further be heated intensification again, heat can pass to rapidly organic adsorbate, makes organic adsorbate quick desorption in duct, with steam from the adsorbent surface desorption out.In addition for the adsorbent of high-k, can the Fast Heating adsorbent, make its surperficial organic molecule desorption.The organic matter of desorption and steam, from desorption column flows out, are converted into liquid through condenser, and the liquid obtained enters storage container, in order to later separation, process.In desorption column adsorbent organic matter by desorption fully after, cut off steam vapour amount, pass into nitrogen, under microwave action, in adsorbent, remaining hydrone is under nitrogen drives, desorption goes out adsorption tower emptying, thereby makes adsorbent obtain drying.Desorption adsorbent completely can be recycled in the absorption of organic exhaust gas or organic wastewater.
In operating process, can regulate the amount of steam according to the dielectric constant of adsorbate and adsorbent, if the macromolecule resin that the employing adsorbent is low-k and the molecular sieve of high hydrophobicity are suitably heightened the steam flow; If active carbon or NACF that the adsorbent adopted is high-k, can significantly reduce the steam vapour amount passed into.In addition, the polarity size of adsorbate also affects the steam intake.If the organic matter of desorption is nonpolar, can suitably increase the water vapour amount; If the organic matter of desorption is strong polarity, can suitably reduce steam vapour amount.Those skilled in the art can regulate voluntarily according to actual conditions.
Being a little of the desorption technology that the present invention proposes: (1), by microwave reinforced steam, makes steam keep the high-temperature steam state, can significantly reduce the consumption of steam, reduces the segregational load of follow-up organic matter and water, has the meaning of energy-saving and emission-reduction; (2) after water vapour enters in the adsorbent duct, under microwave action, can pass to heat rapidly the organic molecule of absorption, significantly improve the desorption rate of organic molecule; (3) steam is introduced, and can reduce localized hyperthermia focus and the spark of active carbon class adsorbent under microwave action, protection sorbent structure, the security that improves device; (4) under microwave action and nitrogen blowing, can realize that adsorbent is dry fast, omitted the unit operations of heated air drying and cold air cooling in single steam desorption, reduced energy consumption.(5) this cover technology is applicable to having the desorption of all kinds of differing dielectric constant adsorbents and polarity adsorbate, has versatility widely;
(4) accompanying drawing explanation
Fig. 1: steam of the present invention is worked in coordination with desorption by microwave device schematic diagram.
In Fig. 1,1-steam evaporator; 2-condenser; 3-condensed fluid reservoir vessel; 4-muff; 5-microwave generator; 6-desorption column; 7-nitrogen gas generator.
In Fig. 2: embodiment 1, NACF surface toluene is at the comparison diagram of different desorption method Toluene residual rates.
In Fig. 3: embodiment 2, Y zeolite surface toluene is at the comparison diagram of different desorption method Toluene residual rates.
In Fig. 4: embodiment 3, the poly-surperficial toluene of divinylbenzene (PDVB) of porous polymer resin is at the comparison diagram of different desorption method Toluene residual rates.
(5) specific embodiment
Below with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to this.
Embodiment 1:
Get NACF 2 grams, absorption toluene 2 grams, the desorption column of packing into, as Fig. 1 mode is built desorption apparatus.Be provided with microwave generator 5 in desorption column 6, steam generator 1 is communicated with the vapour inlet on desorption column 6 tops by flowmeter, nitrogen gas generator 7 is connected with the nitrogen inlet on desorption column 6 tops by flowmeter, nitrogen outlet and vapor outlet port are located at respectively desorption column 6 bottoms, vapor outlet port is communicated with condenser 2, condenser 2 outlets connect a storage container 3, organic matter and the water of the liquid state that storage condenses from condenser.Pipeline between the vapour inlet on steam generator 1 and desorption column 6 tops is provided with muff 4 outward, prevents steam condensing.
Carry out desorption by following three kinds of methods:
(1) microwave+steam: from desorption column top vapour inlet, pass into steam, steam flow 1.0g/min, open microwave generator, microwave power is 600W, carry out the desorption processing, the organic matter of desorption and steam flow out from desorption column bottom vapor outlet port, enter condenser condenses, tracking and monitoring Residual Toluene rate, complete to desorption; Then cut off steam, from desorption column top nitrogen inlet, pass into nitrogen, the bottom nitrogen outlet flows out nitrogen, nitrogen air speed 2000h
-1, microwave power is 600W, carries out drying and processes 3 minutes, stops microwave generator and cuts off nitrogen, obtains the adsorbent after desorption; ;
(2) microwave+nitrogen: pass into nitrogen from desorption column top nitrogen inlet, the bottom nitrogen outlet flows out nitrogen, nitrogen air speed 2000h
-1, microwave power is 600W, tracking and monitoring Residual Toluene rate is complete to desorption;
(3) steam, pass into steam from desorption column top vapour inlet, steam flow 1.0g/min, carry out the desorption processing, the organic matter of desorption and steam flow out from desorption column bottom vapor outlet port, enter condenser condenses, tracking and monitoring Residual Toluene rate, complete to desorption; .
Above three kinds of mode desorption rate comparing results are shown in Fig. 2, and result shows, under microwave action, NACF surface toluene can 2 minutes within desorption complete, under steam and microwave cooperating effect, than single microwave, desorption rate is faster.But adopt single steam desorption, need nearly 30 minutes ability desorptions more complete.Therefore, the larger activated carbon fiber adsorbing substance for dielectric constant, microwave can obviously improve desorption rate, and the collaborative microwave of steam can further be accelerated desorption rate, and the absorption residue is seldom.
Embodiment 2:
Get Y zeolite 2 grams, absorption toluene 2 grams, the desorption by microwave tower of packing into, carry out desorption according to three kinds of methods of embodiment 1: (1) microwave+steam, microwave power is 600W, steam flow 1.0g/min; (3) microwave+nitrogen, nitrogen air speed 2000h
-1; (2) steam, steam flow 1.0g/min.
Above three kinds of mode desorption rate comparing results are shown in Fig. 3, and result shows, under microwave action, Y molecular sieve surface toluene can 10 minutes within desorption complete.And under steam and microwave cooperating effect than single microwave, desorption rate is faster, can be complete with regard to desorption within 7 minutes.But adopt single steam desorption, need nearly 30 minutes ability desorptions more complete.Therefore, for the Y molecular sieve adsorbent that certain polarity is arranged, microwave can obviously improve desorption rate, and the collaborative microwave technology of steam can further be accelerated desorption rate, and the absorption residue seldom.
Embodiment 3:
Get poly-divinylbenzene (PDVB) 2 grams of porous polymer resin, absorption toluene 10 grams, the desorption by microwave tower of packing into, carry out desorption according to three kinds of methods of embodiment 1: (1) microwave+steam, microwave power is 600W, steam flow 1.0g/min; (3) microwave+nitrogen, nitrogen air speed 2000h
-1; (2) steam, steam flow 1.0g/min.
Above three kinds of mode desorption rate comparing results are shown in Fig. 4, find, under single microwave action, resin surface toluene desorption rate is very slow, and after 30 minutes, desorption rate only reaches 40%.And under steam and microwave cooperating effect than single microwave, desorption rate significantly improves, can be complete with regard to desorption within 5 minutes.But adopt single steam desorption, need nearly 30 minutes ability desorptions more complete.Therefore, for nonpolar and macromolecule resin adsorbent low-k, single microwave does not have the desorption effect, but the collaborative microwave technology of steam can significantly improve desorption rate, and the absorption residue seldom.
Claims (4)
1. the desorption process for regenerating of an Adsorption of Organic agent, it is characterized in that described method is: be provided with in the desorption and regeneration device of Adsorption of Organic agent of microwave generator in desorption column, there is organic adsorbent to be placed in desorption column the absorption for the treatment of desorption, pass into steam from desorption column top vapour inlet, open microwave generator, microwave power is 500-10000W, carrying out desorption processes 2～30 minutes, the organic matter of desorption and steam flow out from desorption column bottom vapor outlet port, enter condenser condenses; Then cut off steam, from desorption column top nitrogen inlet, pass into nitrogen, the bottom nitrogen outlet flows out nitrogen, and microwave power is 200-2000W, carries out drying processing 2-20 minute, stops microwave generator and cuts off nitrogen, obtains the adsorbent after desorption.
2. the method for claim 1, is characterized in that 0.2-5.0 that volume that described steam per hour passes into is the adsorbent volume doubly.
3. the method for claim 1, the air speed that it is characterized in that described nitrogen is 500-5000h
-1.
4. the desorption and regeneration device of an Adsorption of Organic agent, it is characterized in that described device comprises desorption column, steam generator, nitrogen gas generator, condenser, and be located at the microwave generator in desorption column, described steam generator is communicated with the vapour inlet on desorption column top by flowmeter, nitrogen gas generator is connected with the nitrogen inlet on desorption column top by flowmeter, nitrogen outlet and vapor outlet port are located at respectively the desorption column bottom, and vapor outlet port is communicated with condenser.
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Cited By (17)
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| CN104388111A (en) * | 2014-11-30 | 2015-03-04 | 东北电力大学 | Recovering process of light oil of dry distilled gas of oil shale by virtue of microwave adsorption and desorption |
| CN104479726A (en) * | 2014-11-30 | 2015-04-01 | 东北电力大学 | Microwave-adsorption/desorption oil shale distillation methane light oil recovery device |
| CN106925246A (en) * | 2017-05-11 | 2017-07-07 | 重庆工商大学 | A kind of micro wave regeneration processing method of Powder ash adsorption material |
| CN106975471A (en) * | 2017-05-11 | 2017-07-25 | 重庆工商大学 | A kind of ozone encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN106994337A (en) * | 2017-05-11 | 2017-08-01 | 重庆工商大学 | A kind of micro wave regeneration method of flyash under ultrasonic pretreatment |
| CN107081142A (en) * | 2017-05-11 | 2017-08-22 | 重庆工商大学 | A kind of fluorine gas encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN107096518A (en) * | 2017-05-11 | 2017-08-29 | 重庆工商大学 | A kind of chlorine encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN107096517A (en) * | 2017-05-11 | 2017-08-29 | 重庆工商大学 | Nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN108101312A (en) * | 2017-12-30 | 2018-06-01 | 华电煤业集团有限公司 | A kind of system of the wastewater treatment containing aromatic hydrocarbons |
| CN108993460A (en) * | 2018-07-18 | 2018-12-14 | 罗诚 | The micro wave regeneration mobile layer furnace of activated carbon filter layer in a kind of Industrial cleaning facility equipment |
| CN109701508A (en) * | 2019-02-19 | 2019-05-03 | 安徽国孚凤凰科技有限公司 | The device and its process of desorption and regeneration after a kind of absorption of adsorbent |
| CN110252269A (en) * | 2019-06-13 | 2019-09-20 | 江苏南大环保科技有限公司 | A kind of resin regeneration method for handling containing high-boiling components waste water |
| WO2020034278A1 (en) * | 2018-08-16 | 2020-02-20 | 无锡四方集团有限公司 | In-situ desorption regeneration process of adsorbent adsorbing organic waste gas |
| CN111396900A (en) * | 2020-03-30 | 2020-07-10 | 浙江工业大学 | Device and process for microwave-assisted catalytic combustion of high-concentration grease wastewater |
| CN112691653A (en) * | 2020-12-22 | 2021-04-23 | 广东电网有限责任公司电力科学研究院 | Regeneration treatment method of adsorbent for transformer oil |
| CN113244771A (en) * | 2021-03-31 | 2021-08-13 | 大连亚泰科技新材料股份有限公司 | Regenerating unit of sterilization inactivation air purification agent |
| CN113445571A (en) * | 2020-03-24 | 2021-09-28 | 欧军飞 | Method for improving water vapor collection efficiency of MOF-801 from unsaturated air |
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| CN104388111A (en) * | 2014-11-30 | 2015-03-04 | 东北电力大学 | Recovering process of light oil of dry distilled gas of oil shale by virtue of microwave adsorption and desorption |
| CN104479726A (en) * | 2014-11-30 | 2015-04-01 | 东北电力大学 | Microwave-adsorption/desorption oil shale distillation methane light oil recovery device |
| CN104388111B (en) * | 2014-11-30 | 2016-04-06 | 东北电力大学 | A kind of recovery process of microwave adsorption desorption oil shale distillation gas lightweight oil |
| CN106925246A (en) * | 2017-05-11 | 2017-07-07 | 重庆工商大学 | A kind of micro wave regeneration processing method of Powder ash adsorption material |
| CN106975471A (en) * | 2017-05-11 | 2017-07-25 | 重庆工商大学 | A kind of ozone encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN106994337A (en) * | 2017-05-11 | 2017-08-01 | 重庆工商大学 | A kind of micro wave regeneration method of flyash under ultrasonic pretreatment |
| CN107081142A (en) * | 2017-05-11 | 2017-08-22 | 重庆工商大学 | A kind of fluorine gas encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN107096518A (en) * | 2017-05-11 | 2017-08-29 | 重庆工商大学 | A kind of chlorine encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN107096517A (en) * | 2017-05-11 | 2017-08-29 | 重庆工商大学 | Nitrogen dioxide encloses the micro wave regeneration method of lower flyash with carbon dioxide mix atmosphere |
| CN108101312A (en) * | 2017-12-30 | 2018-06-01 | 华电煤业集团有限公司 | A kind of system of the wastewater treatment containing aromatic hydrocarbons |
| CN108993460A (en) * | 2018-07-18 | 2018-12-14 | 罗诚 | The micro wave regeneration mobile layer furnace of activated carbon filter layer in a kind of Industrial cleaning facility equipment |
| CN108993460B (en) * | 2018-07-18 | 2021-04-13 | 南通市金宏电化设备有限公司 | Microwave regeneration moving layer furnace of active carbon filter layer in industrial purification equipment |
| WO2020034278A1 (en) * | 2018-08-16 | 2020-02-20 | 无锡四方集团有限公司 | In-situ desorption regeneration process of adsorbent adsorbing organic waste gas |
| CN109701508A (en) * | 2019-02-19 | 2019-05-03 | 安徽国孚凤凰科技有限公司 | The device and its process of desorption and regeneration after a kind of absorption of adsorbent |
| CN110252269A (en) * | 2019-06-13 | 2019-09-20 | 江苏南大环保科技有限公司 | A kind of resin regeneration method for handling containing high-boiling components waste water |
| CN113445571A (en) * | 2020-03-24 | 2021-09-28 | 欧军飞 | Method for improving water vapor collection efficiency of MOF-801 from unsaturated air |
| CN111396900A (en) * | 2020-03-30 | 2020-07-10 | 浙江工业大学 | Device and process for microwave-assisted catalytic combustion of high-concentration grease wastewater |
| CN112691653A (en) * | 2020-12-22 | 2021-04-23 | 广东电网有限责任公司电力科学研究院 | Regeneration treatment method of adsorbent for transformer oil |
| CN112691653B (en) * | 2020-12-22 | 2023-07-04 | 广东电网有限责任公司电力科学研究院 | Regeneration treatment method of adsorbent for transformer oil |
| CN113244771A (en) * | 2021-03-31 | 2021-08-13 | 大连亚泰科技新材料股份有限公司 | Regenerating unit of sterilization inactivation air purification agent |
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Application publication date: 20131218 |